超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速检测茶叶及其制品中35种合成色素

Rapid determination of 35 kinds of synthetic pigments in tea and its products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

中文关键词:  超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法  快速检测  合成色素

英文关键词:ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry  rapid determination  synthetic pigment  tea and its products

中文摘要:

      目的 建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定茶叶及其制品中35种合成色素的方法。方法 样品经5%氨水甲醇溶液超声提取, 采用C18为材料净化, 一定比例稀释后, 经Waters Acquity UPLC BEH C18 色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 以5 mmol/L乙酸铵水溶液和甲醇作为流动相, 进行梯度洗脱。采用电喷雾离子源负离子电离模式, 一级母离子全扫描和数据依赖的二级子离子扫描模式进行质谱检测, 同时获得一级母离子和二级碎片子离子的高质量精度质谱数据。通过与自建数据库检索比对进行初步筛查, 发现可疑样品再与标准品二级谱图比对确证, 外标法定量。结果 本方法在无标准品的情况下可实现对茶叶及其制品中35种合成色素快速筛查, 有标准品的情况下无需基质标准曲线即可实现准确定性和定量, 方法检出限为0.02~2.97 mg/kg, 3水平加标试验的平均回收率为71.4%~117.7%, 相对标准偏差为0.1%~15.3%, 采用本方法对市售实际样品进行检验, 9批次样品分别检出柠檬黄、日落黄和亮蓝。结论 该方法通量高、速度快、成本低, 可用于茶叶及其制品中35种合成色素的快速定性和定量检测。

英文摘要:

      Objective To establish a method for the determination of 35 kinds of synthetic pigments in tea and its products by ultra performance liquid chromatography-quadrupole/electrostatic field orbital trap high resolution mass spectrometry. Methods Samples were extracted by ultrasound with 5% ammonia methanol solution, purified by C18, diluted at a certain ratio, and separated by Waters Acquity UPLC BEH C18 chromatographic column (100 mm × 2.1 mm, 1.7 μm). Gradient elution was carried out with 5 mmol/L ammonium acetate aqueous solution and methanol as mobile phase. The electrospray ion source negative ion ionization mode, primary parent ion full scanning mode and data-dependent secondary daughter ion scanning mode were used for mass spectrometry detection, and high quality precision mass spectrometry data of primary parent ion and secondary fragment ion were obtained. Through the search and comparison with the self-built database, the preliminary screening was conducted, and the suspicious sample was found and confirmed by the secondary spectrum comparison with the standard product, and the quantitative method was external standard. Results The method could quickly screen 35 kinds of synthetic pigments in tea and its products without standard products, and could achieve accurate qualitative and quantities results without matrix standard curve in the case of standard products. The limits of detection of the compounds were 0.02–2.97 mg/kg. The average recoveries of 3 different spiked levels were 71.4%–117.7%, and the relative standard deviation were 0.1%–15.3%. This method was applied to analyze the actual samples on the market, and tartrazine, sunset yellow and brilliant blue were detected in 9 batches of samples respectively. Conclusion The method has high throughput, high speed and low cost, and can be used for rapid qualitative and quantitative determination of 35 kinds of synthetic pigments in tea and its products.